CN113363482B - Composite binder for silicon-based negative electrode of lithium ion battery and preparation method and application thereof - Google Patents

Composite binder for silicon-based negative electrode of lithium ion battery and preparation method and application thereof Download PDF

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CN113363482B
CN113363482B CN202110447517.5A CN202110447517A CN113363482B CN 113363482 B CN113363482 B CN 113363482B CN 202110447517 A CN202110447517 A CN 202110447517A CN 113363482 B CN113363482 B CN 113363482B
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lithium ion
ion battery
silicon
negative electrode
electrode
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CN113363482A (en
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吴曙星
林展
杨雅君
邱钧城
肖华艳
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Guangdong University of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621—Binders
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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Abstract

The invention belongs to the technical field of lithium ion batteries, and discloses a composite binder for a silicon-based negative electrode of a lithium ion battery, a preparation method and application thereof, wherein the composite binder is abbreviated as C-SP-CA and is prepared by uniformly dispersing sericin powder in deionized water, adding citric acid to form a mixed solution, and carrying out in-situ crosslinking reaction at 120-160 ℃. Sericin in the adhesive is composed of a large amount of amino acids such as serine and aspartic acid with hydrophilic groups on side chains, and has better dispersibility compared with the traditional PVDF adhesive. In addition, the formed three-dimensional network structure is beneficial to the transmission of electrons and ions, and the mechanical property of the binder is greatly improved, so that the electrode keeps good integrity in the circulating process. The binder prepared by the method can obviously improve the electrochemical performance of the silicon-based cathode of the lithium ion battery, and in addition, the binder has the advantages of simple preparation process, low cost and the like, and easily meets the requirement of industrialization.

Description

Composite binder for silicon-based negative electrode of lithium ion battery and preparation method and application thereof
Technical Field
The invention belongs to the technical field of lithium batteries, and particularly relates to a silicon-based (SiO) lithium ion battery x ) A composite binder of a negative electrode, a preparation method and application thereof.
Background
With the constant popularization of new energy electric vehicles, lithium ion batteries with high energy density become the direction of future development of power batteries. At present, the commercial lithium ion battery cathode material is mainly graphite, but the lower theoretical capacity (372 mAh g) is realized -1 ) It is difficult to meet the demand for high energy density. Elemental silicon has a relatively high capacity (4200 mAh g) -1 ) However, during the process of lithium ion desorption/intercalation, huge volume expansion of up to 300% occurs, causing silicon particles to crack and pulverize, seriously affecting the cycle life of the electrode. Silicon monoxide (SiO) compared to elemental silicon x ，0<x<2) Has considerable theoretical capacity (1500 mAh g) -1 ) And small volume change (100-150%) are the most commercially promising high performance anode materials. However, siO due to a not negligible volume expansion (about 200%) SiO x The cathode material also faces fatality such as rapid capacity attenuation and poor stabilityAnd (5) a defect.
The adhesive is one of important constituent materials of the lithium ion battery, can adhere active material particles and conductive agent particles on a current collector, maintains the structural integrity of an electrode in the charge and discharge process, and has important influence on improving the cycle stability of the lithium ion battery. Therefore, the multifunctional composite binder is synthesized by improving SiO x Electrochemical performance, the most economical and effective method for realizing high energy density lithium batteries.
Polyvinylidene fluoride (PVDF) is the most widely used commercial binder at present and has good electrochemical stability. However, in the face of SiO with high energy density x In the case of the negative electrode material, PVDF and SiO x The particles form weak van der Waals forces and are difficult to bear SiO x The stress generated by the volume expansion of the particles in the circulation process is easy to cause the damage of the electrode structure.
Sericin as a natural high molecular protein has good water solubility and dispersibility and is a promising SiO x And (3) a negative electrode binder. However, the single sericin has a linear structure, poor adhesion property, and difficulty in maintaining SiO x The volume of the particles expands during the cycle. Based on the method, the composite adhesive with a three-dimensional network structure is designed through the in-situ crosslinking reaction of sericin and micromolecular citric acid, the mechanical strength of the adhesive is improved, and SiO is realized x Cycling stability of the negative electrode.
Disclosure of Invention
In order to solve the problem that the adhesive in the prior art is difficult to solve the problem of high energy density SiO x The invention aims to provide a silicon-based (SiO) for a lithium ion battery x ) And (3) a composite binder of the negative electrode. The binder and SiO x The particle surface has rich binding sites, and the mechanical strength of the adhesive is enhanced to a great extent by forming strong covalent bond effect among crosslinking reactions, so that SiO can be effectively inhibited x The electrode has the problem of volume expansion in the circulation process, so that SiO x The electrode has a stable cycling behavior.
Another aspect of the present inventionAims to provide the SiO used for the lithium ion battery x The preparation method of the composite binder of the negative electrode comprises the step of synthesizing the composite binder of a three-dimensional network structure through in-situ crosslinking.
Still another object of the present invention is to provide the above SiO for lithium ion batteries x Application of composite binder of negative electrode.
The purpose of the invention is realized by the following technical scheme:
silicon-based (SiO) for lithium ion battery x ) The composite binder of the negative electrode is prepared by uniformly dispersing sericin powder in deionized water, adding citric acid to form a mixed solution, and carrying out in-situ crosslinking reaction at 120-160 ℃.
Preferably, the mass ratio of the sericin powder to the citric acid is (1-2): 1.
Preferably, the volume ratio of the sericin powder to the deionized water is (20-30) mg:1mL.
The composite binder is used for preparing SiO of the lithium ion battery x A method of making a negative electrode, comprising the steps of:
s1, adding sericin powder and citric acid into deionized water, and stirring until the sericin powder and the citric acid are completely dissolved to obtain a mixed solution;
s2, adding an electrode active substance SiO into the mixed solution x Mixing and stirring the mixture and a conductive agent to obtain uniformly dispersed electrode slurry;
s3, coating the obtained electrode slurry on a current collector, heating at 120-150 ℃, and promoting the sericin powder and citric acid to perform a crosslinking reaction in the heating process to obtain the silicon-based negative electrode of the lithium ion battery, namely SiO x Negative electrode of which 0<x<2。
Preferably, the stirring time in step S2 is 6 to 8 hours.
Preferably, the conductive agent in step S2 is one or more of Super P, acetylene black, carbon nanotubes, or carbon black.
Preferably, the SiO in step S2 x 70-80 wt% of the electrode slurry, 10-20 wt% of the conductive agent of the total mass of the electrode slurry, and mixingThe solution accounts for 5-10 wt% of the total mass of the electrode slurry.
Preferably, the heating time in step S3 is 120 to 360min.
Silicon-based (SiO) lithium ion battery x ) The cathode is prepared by the method.
The composite binder is applied to lithium ion batteries.
The invention adopts natural high molecular protein sericin as a main chain to be crosslinked with micromolecule citric acid to obtain the composite binder with a three-dimensional network structure. Under a certain temperature condition, the imino group of the sericin and the carboxyl group of the citric acid can generate a cross-linking reaction to generate the composite adhesive with a three-dimensional network structure. Sericin in the adhesive consists of a large number of amino acids such as serine and aspartic acid with hydrophilic groups on side chains, and has better dispersibility compared with the traditional PVDF adhesive. In addition, the formed three-dimensional network structure is beneficial to the transmission of electrons and ions, and the mechanical property of the binder is greatly improved, so that the electrode keeps good integrity in the circulation process. The adhesive prepared by the method can remarkably improve SiO content of the lithium ion battery x The electrochemical performance of the cathode, in addition, the preparation process of the binder is simple, the cost is low, and the like, and the industrial requirement is easy to achieve.
Compared with the prior art, the invention has the following beneficial effects:
1. the composite binder has a three-dimensional network structure, and the binder selects natural high-molecular protein sericin as a main chain of the binder to be crosslinked with micromolecular citric acid, so that the composite binder with the three-dimensional network structure is accurately regulated and controlled. The adhesive is used in silicon-based SiO x In the electrode, siO is greatly improved x Cycling stability of the electrode.
2. The composite binder prepared by the invention is a water-based binder, has the advantages of environmental friendliness and low cost, and has wide raw material sources and low price compared with the traditional PVDF. The sericin powder is a natural polysaccharide substance, is composed of various amino acids such as glycine and serine, contains rich carboxyl and amino, and has the advantages of low price, good dispersibility, water solubility and the like.
3. SiO of the composite binder of the invention x The catalyst still maintains good cycling stability under higher loading capacity and has important commercial value.
Drawings
Fig. 1 is a graph showing cycle performance of the lithium ion battery prepared in application example 1.
FIG. 2 shows SiO after the lithium ion battery in application example 2 circulates for 100 cycles x SEM image of the electrode.
Fig. 3 is a graph comparing the cycle performance of the lithium ion batteries prepared in application example 2 with those prepared in comparative example 1 and comparative example 2.
Detailed Description
The following examples are presented to further illustrate the present invention and should not be construed as limiting the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. The reagents, methods and apparatus employed in the present invention are conventional in the art, except as otherwise indicated.
Example 1
SiO for lithium ion battery x The composite binder of the negative electrode is prepared by uniformly dispersing sericin powder and citric acid in deionized water according to a mass ratio of 1.
Example 2
SiO for lithium ion battery x The composite binder of the negative electrode is prepared by uniformly dispersing sericin powder and citric acid in deionized water according to a mass ratio of 2.
Example 3
SiO for lithium ion battery x The composite binder of the negative electrode is prepared by uniformly mixing sericin powder and citric acid according to a mass ratio of 1.5Dispersing in deionized water to obtain mixed solution with the concentration of 25mg/mL, and carrying out in-situ crosslinking at 160 ℃ to obtain the composite binder with the three-dimensional network structure.
Application example 1
1. Uniformly dispersing sericin powder and citric acid in deionized water according to a mass ratio of 1;
2. mixing SiO x Adding the material and a conductive agent Super P into the mixed solution according to the mass ratio of 7;
3. coating the electrode slurry on a copper foil, carrying out in-situ crosslinking at 150 ℃ to form a composite binder with a three-dimensional network structure, carrying out vacuum drying and slicing to prepare SiO x (0<x<2) And a negative electrode sheet.
Fig. 1 is a graph showing cycle performance of the lithium ion battery prepared in application example 1. As can be seen from FIG. 1, siO x (0<x<2) The current density of the electrode is 500mAg -1 Then, after 300 cycles, the discharge capacity reaches 960mAh g -1 Description of SiO x The negative electrode exhibits excellent cycle stability.
Application example 2
1. Dissolving sericin powder and citric acid particles in deionized water according to a mass ratio of 1;
2. then SiO x And adding the material and the conductive agent Super P into the mixed solution according to the mass ratio of 7. Wherein the dosage of the mixed solution accounts for 10 percent of the mass of the electrode;
3. coating the electrode slurry on a copper foil, heating at 150 ℃ for 120min for in-situ crosslinking to form a composite binder with a three-dimensional network structure, and transferring the composite binder into an oven at 80 ℃ for full drying to obtain SiO x (0<x<2) And a negative electrode sheet.
4. Transferring the dried cathode electrode piece into a glove box filled with argon, taking a lithium piece as a counter electrode, and taking 1mol/L LiPF as electrolyte 6 As solute, solvent was EC and DEC in a volume ratio of 1, with 10wt% fec and 1wt% vc as additives. Using CR2032 buttonAnd (3) assembling the button cell, standing the assembled button cell for 8 hours, and carrying out constant current test on the electrochemical performance of the battery after standing in a blue test system. Since a cross-linking reaction occurs between Sericin (SP) and Citric Acid (CA), the mechanical strength of the binder is enhanced.
FIG. 2 shows SiO after the lithium ion battery in application example 2 circulates for 100 cycles x SEM image of the electrode. As can be seen from fig. 2, after the electrode using the C-SP-CA binder is cycled for 100 cycles, the surface of the electrode is flat and has no cracks, which indicates that the C-SP-CA binder can effectively maintain the integrity of the electrode, thereby improving the cycling stability of the electrode. Fig. 3 is a graph comparing the cycle performance of the lithium ion batteries prepared in application example 2 and comparative examples 1 and 2. As can be seen from FIG. 3, at a current density of 200mA g -1 SiO prepared using C-SP-CA Binder x (0<x<2) The discharge capacity of the electrode is 1134.4mAh g after 90 cycles of circulation -1 Whereas the discharge capacities using sericin only in comparative example 1 and carboxymethyl cellulose only in comparative example 1 were 40.7mAh g, respectively -1 And 949.4mAh g -1 Description of SiO prepared in application example 2 x The electrode has higher specific discharge capacity and better cycling stability.
Comparative example 1
1. Dissolving sericin powder in deionized water to obtain a yellowish mixed solution with the concentration of 20 mg/mL;
2. then SiO x And adding the materials and the conductive agent into the mixed solution according to the mass ratio of 7. Wherein the dosage of the mixed solution accounts for 10 percent of the mass of the electrode.
3. And (3) coating the electrode slurry on a copper foil, and fully drying in an oven at 80 ℃ to obtain the negative electrode plate.
4. Transferring the dried cathode electrode plate into a glove box filled with argon, taking a lithium plate as a counter electrode, and using 1mol/LLIPF as electrolyte 6 As solute, solvent was EC and DEC in a volume ratio of 1, with 10wt% fec and 1wt% vc as additives. The button cell was assembled using a CR2032 button cell and the assembled button cell was left to stand for 8h. The standing battery is subjected to constant current test electrochemistry in a blue light test systemCan be used.
Comparative example 2
1. 20mg of carboxymethyl cellulose (CMC) is dissolved in 1mL of deionized water to obtain a viscous mixed liquid with the concentration of 20 mg/mL;
2. then SiO x And adding the materials and the conductive agent into the mixed solution according to the mass ratio of 7. Wherein the dosage of the mixed solution accounts for 10 percent of the mass of the electrode.
3. And (3) coating the electrode slurry on a copper foil, and fully drying in an oven at 80 ℃ to obtain the negative electrode plate.
4. Transferring the dried negative electrode plate into a glove box filled with argon, taking a lithium plate as a counter electrode, and using 1M LiPF as electrolyte 6 As solutes, solvents were EC and DEC at a volume ratio of 1, with 10wt% fec and 11wt% vc as additives. And assembling the button cell by using a CR2032 button cell, standing the assembled button cell for 8 hours, and carrying out constant current test on the electrochemical performance of the battery after standing in a blue-ray test system.
As can be shown by the above application example 2 and comparative examples 1 and 2, the C-SP-CA binder of the present invention has good mechanical properties, can ensure the integrity of the electrode during the cycle, and produces SiO x (0<x<2) After 90 cycles of electrode circulation, the discharge capacity can reach 1134.4mAh g -1 SiO prepared as described above x The electrode has higher specific discharge capacity and better cycling stability, and SiO of C-SP-CA adhesive is used x The electrode exhibits excellent electrochemical performance.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.

Claims (5)

1. A composite binder for a silicon-based cathode of a lithium ion battery is characterized in that the composite binder is abbreviated as C-SP-CA and is prepared by uniformly dispersing sericin powder in deionized water, adding citric acid to form a mixed solution, and carrying out in-situ crosslinking reaction at 120-160 ℃; the mass ratio of the sericin powder to the citric acid is (1-2) to 1, and the volume ratio of the sericin powder to the deionized water is (20-30) mg to 1mL.
2. The method for preparing the silicon-based negative electrode of the lithium ion battery by using the composite binder as claimed in claim 1, is characterized by comprising the following steps of:
s1, adding sericin powder and citric acid into deionized water, and stirring until the sericin powder and the citric acid are completely dissolved to obtain a mixed solution;
s2, adding an electrode active substance SiO into the mixed solution x Mixing and stirring the mixture and a conductive agent for 6 to 8 hours to obtain uniformly dispersed electrode slurry; the SiO x 70-80 wt% of the total mass of the electrode slurry, 10-20 wt% of the total mass of the electrode slurry and 5-10 wt% of the total mass of the electrode slurry;
s3, coating the obtained electrode slurry on a current collector, heating at 120-150 ℃ for 120-360 min, and promoting the sericin powder and citric acid to perform a crosslinking reaction in the heating process to obtain the silicon-based negative electrode of the lithium ion battery, namely the SiO x Negative electrode of which 0<x<2。
3. The method for preparing the silicon-based negative electrode of the lithium ion battery by using the composite binder according to claim 2, wherein the conductive agent in the step S2 is one or more of Super P, acetylene black, carbon nanotubes or carbon black.
4. A silicon-based negative electrode for a lithium ion battery, wherein the silicon-based negative electrode for the lithium ion battery is prepared by the method of claim 2 or 3.
5. Use of the composite binder of claim 1 in a lithium ion battery.
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